CN103936510A - Slow release fertilizer suitable for integration of water and fertilizer and preparation method of fertilizer - Google Patents
Slow release fertilizer suitable for integration of water and fertilizer and preparation method of fertilizer Download PDFInfo
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Abstract
The invention provides a slow release fertilizer suitable for integration of water and fertilizer. The slow release fertilizer is a nanocapsule slow release fertilizer formed by using chemical fertilizers as core materials and using slowly soluble polymers as wall materials and can be dispersed in water to form a colloidal solution and achieve the aims of slow release and controlled release. The invention further provides a preparation method of the slow release fertilizer. Capsule wall materials of the slow release fertilizer, namely slowly soluble polymers with opposite charges, are mixed and then carry out polymerization reaction and coat the core materials, and the materials are solidified by a crosslinking agent and are filtered and dried, thus obtaining the nanocapsule slow release fertilizer. The slow release fertilizer can be dispersed in water to form the colloidal solution and can be used for irrigation together with water. The capsule wall materials are the slowly soluble polymers, can be slowly dissolved in soil to achieve the aim of controlled release and can not cause secondary pollution to the soil.
Description
Technical field
The invention belongs to the fertilizer field of farm crop, more precisely relate to a kind of slow release fertilizer being applicable to water-fertilizer integral.
Background technology
Along with the continuous increase of China's population, grain demand is also increasing, and greatly developing agricultural is important measures.Chemical fertilizer plays a part more and more important in agricultural, and present chemical fertilizer in use mainly exists amount of application large, and utilization ratio is low, and soil is polluted to this two large problems.China's water resources lacks, and agriculture water requirement is large, and dry season, lack of water was one of important factor hindering China's agricultural development.So, solution chemical fertilizer utilization ratio, soil pollution have become one of important content of research chemical fertilizer with saving agricultural water problem.China's water resources famine, uses with the agriculture water yield and accounts for 61.9% of total water amount, and annual agricultural water breach is very large, and drought and water shortage has become one of key constraints threatening grain security, restriction agricultural sustainable development.Under this urgent form, China's agricultural development direction need change the intensive style of making rational use of resources into produces, and the Integration of Water into Fertilizer is the inevitable choice of modern agricultural development.Therefore, research can be applicable to water-fertilizer integral, improves chemical fertilizer utilization ratio, reduces fertilizer amount, and the chemical fertilizer that alleviates environmental pressure is current emphasis.
What solve at present these two aspect problems is new type chemical fertilizer---water-soluble fertilizer and slowly-releasing Controlled Release Fertilizer.Water-soluble fertilizer can be dissolved in water, in irrigating, reaches fertilising object with water, is applicable to modern agriculture, but water-soluble fertile release rate is fast, and plant is limited to the absorption of nutrient within a certain period of time, has caused the waste of water-soluble fertilizer, has reduced utilization ratio; Sustained-release and controlled release fertilizer can discharge fertilizer slowly, and the rate of release of its fertilizer nutrient and plant-growth cycle adapt, and utilization ratio is high, and has saved manpower, has reduced the time.But sustained-release and controlled release fertilizer is larger particles, current fertilization mode is artificial or mechanical system, fails to be dissolved in water, reaches the object of fertilising in can not irrigating with water, has wasted manpower and time.
China Patent Publication No. CN102180731A discloses a kind of polymer emulsion coated slow release fertilizer that nano material is carrier and preparation method thereof of take.This scheme is to take hydroxyethyl methylacrylate, vinyl cyanide and starch as raw material, adopt microemulsified and high-shear technology, prepare the heterogeneous mixed polymers of nano level hydroxyethyl methylacrylate-vinyl cyanide-starch, as water-maintaining slowly/controlled releasing fertilizer coating cementing agent and organic-inorganic complex fertilizer adhesive for granulating.This slow-release fertilizer has just used nano material as its coated fertilizer, and the particle of fertilizer is all larger, and in water, solvability is very poor, though reached the object of slowly-releasing, but be not suitable for the application of water-fertilizer integral.
China Patent Publication No. CN101717301A discloses a kind of capsule type microbial fertilizer and preparation method.This scheme is using biological bacteria as core, is carried out micro encapsulation, but wherein gained particle diameter wet, dry capsule is respectively 2.40-3.50mm and 0.8-1.5mm.Though this microorganism fertilizer is encapsulated by fertilizer, reached the effect of slowly-releasing, but its preparation method is that monomer capsule material is mixed with fertilizer, make capsule material carry out absorption fully to fertilizer coated, and particle diameter is larger, can not be effectively dispersed in water and form water-soluble suspension, the application of water-fertilizer integral is had to larger limitation.
China Patent Publication No. CN102731222A discloses a kind of slow controlled release compound fertilizer and preparation method thereof.This scheme is that various fertilizer is carried out to micro encapsulation, and then its mixing is carried out to granulation, because particle is large, poorly soluble in water, is still not suitable for the application of water-fertilizer integral.
According to above-mentioned, the current slow-release fertilizer particle of China is all larger, though can reach the object of Controlled release, is not suitable for modern agriculture water-fertilizer integral, in fertilising process, has wasted a large amount of manpowers and time, has increased the consumption of water.Therefore, in order to adapt to the development of modern agriculture, need further exploitation can be suitable for water-fertilizer integral, can reach again the new-type fertilizer of sustained-release and controlled release.
Summary of the invention
In order to solve above-mentioned deficiency and defect, the present invention proposes a kind of slow-release fertilizer of applicable water-fertilizer integral.This fertilizer is that Nano capsule is fertile, and granularity is little, is dissolved in water and can forms colloidal solution, can irrigate with water; And adopt microcapsule to be coated, can reach the object of Controlled release, single fertilization, the fertile water-saving of time and labour saving province; The material that in this fertilizer, capsule material used is water-soluble, after slowly dissolving in soil, fertilizer slowly releases, and reaches slow release effect, and production technique is simple.
The present invention has further proposed a kind of preparation method of slow-release fertilizer of applicable water-fertilizer integral.This preparation method, after utilizing two kinds of slow soluble polymers with opposite charges to mix, by the pH value of regulation system, reduces the solubleness of capsule material, make it that aggregation occur, parcel core, then add solidifying agent to be cured, filtration drying, obtains Nano capsule slow-release fertilizer.This slow-release fertilizer is coated by delaying soluble polymer, and is nano particle size, and energy rapid dispersion, in water, forms colloidal solution, in being manured into soil together with water.Along with the slow dissolving of slow soluble polymer, fertilizer slowly discharges, and reaches the object of sustained-release and controlled release.
The slow-release fertilizer of a kind of applicable water-fertilizer integral of the present invention, is characterized in that, this slow-release fertilizer is comprised of core and capsule material, wherein core is one or more mixtures in following chemical fertilizer: urea, potassium primary phosphate, primary ammonium phosphate, phosphoric acid one hydrogen ammonia, potassium sulfate, Repone K; Wherein capsule material is the mixture of positively charged polymkeric substance and electronegative soluble polymer.
Positively charged water-soluble polymkeric substance described above is one or more following mixtures: polyene propyl group quaternary ammonium salt, chitosan, gum arabic, cationic starch, cationic polyacrylamide, cationic polyvinyl base pyrrolidone, polyvinylamine, poly-2-ethene tetrahydroglyoxaline, modified cation type water-soluble poly aminoresin, cation water-soluble epoxy resin, polyethylene imine based, polyamine epichlorohydrin resin, heavy is how by-epichlorohydrin resin, methacrylic acid isobutyl alkyl ethyl ester, wherein in positive charge water-soluble polymkeric substance liquid state, add with positive charge water-soluble amount of polymers 10% ~ 20% containing the 30% hydroxyalkyl starch aqueous solution, carry out emulsification, obtain positively charged water-soluble polymer micro-emulsion.
Electronegative water-soluble polymkeric substance described above is one or more following mixtures: gelatin, casein food grade, xanthan gum, hyaluronic acid, carboxymethyl cellulose, carboxymethyl starch, water soluble oxidized starch, phosphate ester starch, anionic polyacrylamide, negatively charged ion Polyvinylpyrolidone (PVP), polymaleic anhydride, negatively charged ion is opened Pu Shi resin, Witco 1298 Soft Acid, sodium laurylsulfonate, sodium cetanesulfonate, anionic water soluble polyurethane resin, wherein in negative charge water-soluble polymkeric substance liquid state, add with negative charge water-soluble polymkeric substance 10% ~ 20% containing the 30% hydroxyalkyl starch aqueous solution, carry out emulsification, obtain electronegative water-soluble polymer micro-emulsion.
The slow-release fertilizer of a kind of applicable water-fertilizer integral of the present invention, is characterized in that the preparation method of this slow-release fertilizer comprises the following steps:
(1), chemical fertilizer and water are dissolved in the ratio of 1:1 ~ 10,3% ~ 10% the polyvalent alcohol nonionic surface active agent that adds again fertilizer amount, utilize high speed lifting stirrer to be mixed into emulsion, setting rotating speed is 800r/min ~ 1200r/min, send into again and in high pressure homogenizer, carry out high-pressure homogeneously twice, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained chemical fertilizer micro emulsion A micro emulsion in step (1) is sent in high speed lifting stirrer, add in proportion again step positively charged water-soluble polymer micro-emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative water-soluble polymer micro-emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1 ~ 2:1 ~ 2:1 ~ 2, utilizing pH adjusting agent to regulate pH value is 3.8 ~ 5.0, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 2% ~ 10%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
Polyvalent alcohol nonionic surface active agent described in above-mentioned steps (1) is one or more following mixtures: sorbitol ester, tween, polyvinyl alcohol, sucrose fatty ester, diethanolamine fatty acid ester, methacrylic acid stearyl ester.
In above-mentioned steps (1), chemical fertilizer is dissolved in water, forms solution, then add 5% ~ 20% emulsifying agent, by high pressure homogenizer, carry out homogeneous.Because capsule material is slow soluble materials, can be dissolved in water, and chemical fertilizer also can be dissolved in and ionizes out zwitterion in water, react cohesion with the capsule material with positive and negative charge, therefore,, in order to prevent reacting of chemical fertilizer and capsule material, guarantee fertilizer efficiency, chemical fertilizer need be dissolved in organic solvent, keep the stability of chemical fertilizer ion; Moreover the present invention makes Nano capsule slow-release fertilizer, but the globule size of capsule is determined by the emulsifying stage particle diameter of liquid, therefore by high pressure homogenizer, make chemical fertilizer become microemulsion, size evenly, guaranteed that follow-up capsule size is below 50nm, and embedding rate can reach more than 90%.
The positively charged water-soluble polymer micro-emulsion adding in above-mentioned steps (2) and the treatment process of electronegative water-soluble polymer micro-emulsion are, by positively charged and water-soluble polymkeric substance negative charge, add respectively 10% ~ 20% the tensio-active agent 30% hydroxyalkyl starch aqueous solution, by high pressure homogenizer, be also to have guaranteed that capsule material can form nano level microemulsion again.Wherein microemulsion is nano level, guarantees follow-up capsule grain diameter; Add tensio-active agent simultaneously, can improve the activity of polymkeric substance, make can fully react with the polymkeric substance of electric charge, increase operation rate.
Solidifying agent described above is one or more following mixtures: methacrylic acid imidazolidyl ketone hydroxyl ethyl ester, glutaraldehyde, Virahol, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2 isopropyl imidazole, diethyl amino propylamine, Triethylenetetramine (TETA), dimethylaminopropylamine.
PH adjusting agent described above is acid-base modifier, and wherein acidity regulator is: citric acid, oxalic acid, tartrate; Alkalinity regulator is sodium hydroxide solution.
In above-mentioned steps (2), first chemical fertilizer micro emulsion A micro emulsion is fully mixed with positively charged water-soluble polymer micro-emulsion, then add electronegative water-soluble polymer micro-emulsion.Because A micro emulsion fully mixes with positively charged water-soluble polymer micro-emulsion, positively charged water-soluble polymer micro-emulsion is evenly distributed on around A micro emulsion, add after electronegative water-soluble polymer micro-emulsion, after positively charged water-soluble polymer micro-emulsion mixes with electronegative water-soluble polymer micro-emulsion, positive and negative charge combines, there is aggregation, coated core; Regulate again pH value, reduce the solubleness of wall material, it is separated out on core, form capsule; Add solidifying agent, capsule is solidified, strengthened capsule equipment structure, reach good intensity, cracky not, redeposition is separated out, washing, filtration drying, can obtain Nano capsule slow-release fertilizer.
High pressure homogenizer described in above-mentioned steps (1) is electromechanical type convection current high pressure homogenizer, in homogeneous chamber, be provided with two fluid channels, left and right, utilize distinctive Y-shaped structure, make the material convection current of high-pressure solution high speed motion from colliding, be ground into nanometer micro emulsion.
High speed lifting stirrer described in above-mentioned steps (1) (2) (3) is two guide pillar hydraulic lifting stirrers.Hydraulic lifting stirrer, utilizes motor to carry out speed governing, and material, under the high speed rotating effect of blade, acutely stirs up and down in container, produces percussion and shearing with blade, makes aggregate disruption reach rapid dispersion, intimate mixing.Filter type in above-mentioned steps (6) is centrifuging, adopts electric centrifuge, utilizes centrifugal force, carries out solid-liquid separation, obtains required Nano capsule solid.
The present invention is a kind of is applicable to the slow-release fertilizer with water-fertilizer integral, it is characterized in that chemical fertilizer by abundant microemulsified, then micro encapsulation, become Nano capsule.At present the slow-release fertilizer of China is mainly coat fertilizer, also have fertilizer is made into microcapsule, but the fertile particle of coat fertilizer and microcapsule is all larger, irrigate easy blocking pipe together with water.But Nano capsule and microcapsule are except the difference of size, also different at aspects such as capsule material, dispersivenesses.Microcapsules Size is generally larger, be dispersed in water as suspension liquid, as dealt with improperly, produce precipitation, be easy to blocking pipe, and Nano capsule particle diameter is nanometer, is dispersed in water as colloidal solution, can penetrate plant membrane, enter in vegetable cell and tissue, in tissue, slowly discharge Promoting plant growth.
The outstanding feature of slow-release fertilizer of a kind of applicable water-fertilizer integral of the present invention and preparation method thereof is:
1, the present invention combines the water-soluble of chemical fertilizer and slowly-releasing control-release function, utilizes water miscible polymkeric substance as capsule material, coated chemical fertilizer, and along with the slow dissolving of capsule material, fertilizer efficiency slowly discharges, and reaches the object of sustained-release and controlled release.By chemical fertilizer microemulsified, recycling positive and negative charge polymkeric substance aggregation, parcel chemical fertilizer, can make chemical fertilizer capsule reach nano level, is dispersed in water, and forms colloidal solution, irrigates together with water, and blocking pipe not, is applicable to the modern agriculture of water-fertilizer integral.
2, the capsule material using in the present invention is slow molten polymkeric substance, is dispersed in soil and can effectively slowly dissolves, and the material after water-soluble can not cause secondary pollution to soil.
3, the chemical fertilizer in the present invention, can need to carry out any proportioning according to crop, and the growth rhythm according to crop different times, provides nutrition, promotes plant growth, has improved the utilization ratio of fertilizer, can use again time saving and energy saving water-saving saving of labor together with water.
Embodiment
Below by embodiment, the present invention is described in further detail, but should not be construed as scope authority of the present invention, only limits to following example.
embodiment 1
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea
Capsule material: positively charged water-soluble polymkeric substance: chitosan
Electronegative water-soluble polymkeric substance: hyaluronic acid
The pre-treatment of capsule material:
(1), with positive charge water-soluble polymkeric substance, in liquid chitosan, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), with negative charge water-soluble polymkeric substance, in liquid hyaluronic acid, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), urea and water are dissolved in the ratio of 1:2, add again the polyvalent alcohol nonionic surface active agent Tween-60 that accounts for chemical fertilizer 5%, high speed lifting stirrer is mixed into emulsion, setting rotating speed is 800r/min ~ 1200r/min, is mixed into emulsion, then send in high pressure homogenizer, carry out high-pressure homogeneous, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained urea micro emulsion A micro emulsion in step (1) is sent in high speed lifting stirrer, add in proportion the more positively charged water-soluble polymer shell of step glycan microemulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative polymkeric substance hyaluronic acid micro emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=2:1:1, utilizing pH adjusting agent to regulate pH value is 4.5 ~ 5.0, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, setting rotating speed is 1200r/min ~ 1400r/min, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent glutaraldehyde gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 5%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By urea leaching test, the slow-release fertilizer nutrient of a kind of applicable water-fertilizer integral of the present invention discharges as following table:
| Fertilization time | Fertilizer efficiency leaching yield | Capsule material dissolution rate |
| 24h | 3% | 1% |
| 30d | 65% | 50% |
| 60d | 96% | 80% |
| 90d | Completely dissolve | Completely dissolve |
embodiment 2
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea, potassium primary phosphate, and ratio is urea: potassium primary phosphate=2:1
Capsule material: positively charged water-soluble polymkeric substance: quaternary ammonium starch ethers
Electronegative water-soluble polymkeric substance: negatively charged ion oxidation starch
The pre-treatment of capsule material:
(1), with positive charge water-soluble polymkeric substance, in liquid quaternary ammonium starch ethers, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), with negative charge water-soluble polymkeric substance, in liquid anion oxygen starch, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), by the mixture of urea and potassium primary phosphate, dissolve in the ratio of 1:4 with water, the polyvalent alcohol nonionic surface active agent sucrose fatty ester that adds again chemical fertilizer amount 5%, high speed lifting stirrer is mixed into emulsion, and setting rotating speed is 800r/min ~ 1200r/min, be mixed into emulsion, send into again and in high pressure homogenizer, carry out high-pressure homogeneously, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained urea in step (1) and potassium primary phosphate mixing micro emulsion A micro emulsion are sent in high speed lifting stirrer, add in proportion again positively charged water-soluble polymkeric substance quaternary ammonium starch ethers micro emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative water-soluble polymer anion Sumstar 190 micro emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1:2:2, utilizing pH adjusting agent to regulate pH value is 4.0 ~ 4.5, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, setting rotating speed is 1200r/min ~ 1400r/min, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent glutaraldehyde gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 8%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrient of a kind of applicable water-fertilizer integral of the present invention discharges as following table:
| Fertilization time | Fertilizer efficiency leaching yield | Capsule material dissolution rate |
| 24h | 1% | 0.5% |
| 30d | 57.5% | 40% |
| 60d | 95% | 85% |
| 90d | Completely dissolve | Completely dissolve |
embodiment 3
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: phosphoric acid one hydrogen ammonia
Capsule material: positively charged water-soluble polymkeric substance: cationic polyurethane resin
Electronegative water-soluble polymkeric substance: carboxymethyl starch
The pre-treatment of capsule material:
(1), with positive charge water-soluble polymkeric substance, in liquid cationic polyurethane resin, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), with negative charge water-soluble polymkeric substance, in liquid carboxymethyl starch, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), phosphoric acid one hydrogen ammonia and water are dissolved in the ratio of 1:1, add again the polyvalent alcohol nonionic surface active agent methacrylic acid stearyl ester that accounts for chemical fertilizer 8%, high speed lifting stirrer is mixed into emulsion, setting rotating speed is 800r/min ~ 1200r/min, is mixed into emulsion, then send in high pressure homogenizer, carry out high-pressure homogeneous, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained phosphoric acid one hydrogen ammonia micro emulsion A micro emulsion in step (1) is sent in high speed lifting stirrer, add in proportion again positively charged water-soluble polymer cation urethane resin micro emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative water-soluble polymkeric substance carboxymethyl starch micro emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=2:1:1, utilizing pH adjusting agent to regulate pH value is 4.0 ~ 4.5, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, setting rotating speed is 1200r/min ~ 1400r/min, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent 2 isopropyl imidazole gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 4%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrient of a kind of applicable water-fertilizer integral of the present invention discharges as following table:
| Fertilization time | Fertilizer efficiency leaching yield | Capsule material dissolution rate |
| 24h | 2% | 1% |
| 30d | 60% | 45% |
| 60d | 95% | 80% |
| 90d | Completely dissolve | Completely dissolve |
embodiment 4
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea, ammonium hydrogen phosphate, and ratio is urea: ammonium hydrogen phosphate=1:1
Capsule material: positively charged water-soluble polymkeric substance: cationic polyvinyl pyrrolidone
Electronegative water-soluble polymkeric substance: phosphate ester starch
The pre-treatment of capsule material:
(1), with positive charge water-soluble polymkeric substance, in liquid cationic polyvinyl pyrrolidone, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), with negative charge water-soluble polymkeric substance, in liquid phosphate ester starch, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), by the mixture of urea and potassium primary phosphate, dissolve in the ratio of 1:4 with water, the polyvalent alcohol nonionic surface active agent diethanolamine fatty acid ester that adds again chemical fertilizer amount 5%, high speed lifting stirrer is mixed into emulsion, and setting rotating speed is 800r/min ~ 1200r/min, be mixed into emulsion, send into again and in high pressure homogenizer, carry out high-pressure homogeneously, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained urea micro emulsion A micro emulsion in step (1) is sent in high speed lifting stirrer, add in proportion again positively charged water-soluble polymer cation polyvinylpyrrolidone micro emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative polymkeric substance phosphate ester starch micro emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1:1:1, utilizing pH adjusting agent to regulate pH value is 4.0 ~ 4.5, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, setting rotating speed is 1200r/min ~ 1400r/min, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent glutaraldehyde gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 15%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrient of a kind of applicable water-fertilizer integral of the present invention discharges as following table:
| Fertilization time | Fertilizer efficiency leaching yield | Capsule material dissolution rate |
| 24h | 3% | 0.5% |
| 30d | 63% | 45% |
| 60d | 94% | 85% |
| 90d | Completely dissolve | Completely dissolve |
embodiment 5
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea, primary ammonium phosphate, potassium sulfate, and ratio is urea: primary ammonium phosphate: potassium sulfate=2:2:1
Capsule material: positively charged water-soluble polymkeric substance: gum arabic
Electronegative water-soluble polymkeric substance: xanthan gum
The pre-treatment of capsule material:
(1), with positive charge water-soluble polymkeric substance, in liquid gum arabic, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), with negative charge water-soluble polymkeric substance, in liquid xanthan gum, adding the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), by urea, the mixture of primary ammonium phosphate and potassium sulfate, dissolves in the ratio of 1:5 with water, then adds the polyvalent alcohol nonionic surface active agent sorbitol ester that accounts for chemical fertilizer 6%, high speed lifting stirrer is mixed into emulsion, setting rotating speed is 800r/min ~ 1200r/min, is mixed into emulsion, then send in high pressure homogenizer, carry out high-pressure homogeneous, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), by gained urea in step (1), primary ammonium phosphate, potassium sulfate mixing micro emulsion A micro emulsion is sent in high speed lifting stirrer, add in proportion again positively charged polymkeric substance gum arabic micro emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative polymkeric substance xanthan gum micro emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=2:1:1, utilizing pH adjusting agent to regulate pH value is 4.0 ~ 4.5, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, setting rotating speed is 1200r/min ~ 1400r/min, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent Virahol gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 15%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrient of a kind of applicable water-fertilizer integral of the present invention discharges as following table:
| Fertilization time | Fertilizer efficiency leaching yield | Capsule material dissolution rate |
| 24h | 3% | 2% |
| 30d | 70% | 58% |
| 60d | 98% | 87% |
| 90d | Completely dissolve | Completely dissolve |
In above example, each fertilizer fertilizer in 30 days discharges all≤75%, meets slow-release fertilizer standard.
Claims (9)
1. a slow-release fertilizer for applicable water-fertilizer integral, is characterized in that: this slow-release fertilizer is comprised of core and capsule material, and wherein core is one or more mixtures in following chemical fertilizer: urea, potassium primary phosphate, primary ammonium phosphate, phosphoric acid one hydrogen ammonia, potassium sulfate, Repone K; Wherein capsule material is the mixture of the water-soluble of positively charged polymkeric substance and electronegative polymkeric substance.
2. the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 1, it is characterized in that: wherein said positively charged water-soluble polymkeric substance is one or more following mixtures: polyene propyl group quaternary ammonium salt, sodium alginate, chitosan, gum arabic, cationic starch, cationic polyacrylamide, cationic polyvinyl base pyrrolidone, polyvinylamine, poly-2-ethene tetrahydroglyoxaline, modified cation type water-soluble poly aminoresin, cation water-soluble epoxy resin, polyethylene imine based, polyamine epichlorohydrin resin, heavy is how by-epichlorohydrin resin, methacrylic acid isobutyl alkyl ethyl ester, wherein in positive charge water-soluble polymkeric substance liquid state, add with positive charge water-soluble amount of polymers 10% ~ 20% containing the 30% hydroxyalkyl starch aqueous solution, carry out emulsification, obtain positively charged water-soluble polymer micro-emulsion.
3. the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 1, it is characterized in that: wherein said electronegative water-soluble polymkeric substance is one or more following mixtures: gelatin, casein food grade, xanthan gum, hyaluronic acid, carboxymethyl cellulose, carboxymethyl starch, water soluble oxidized starch, phosphate ester starch, anionic polyacrylamide, negatively charged ion Polyvinylpyrolidone (PVP), polymaleic anhydride, negatively charged ion is opened Pu Shi resin, Witco 1298 Soft Acid, sodium laurylsulfonate, sodium cetanesulfonate, anionic water soluble polyurethane resin, wherein in negative charge water-soluble polymkeric substance liquid state, add with negative charge water-soluble polymkeric substance 10% ~ 20% containing the 30% hydroxyalkyl starch aqueous solution, carry out emulsification, obtain electronegative water-soluble polymer micro-emulsion.
4. the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 1, is characterized in that: the preparation method of this slow-release fertilizer comprises the following steps:
(1), chemical fertilizer and water are dissolved in the ratio of 1:1 ~ 10,3% ~ 10% the polyvalent alcohol nonionic surface active agent that adds again fertilizer amount, utilize high speed lifting stirrer to be mixed into emulsion, setting rotating speed is 800r/min ~ 1200r/min, send into again and in high pressure homogenizer, carry out high-pressure homogeneously twice, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained chemical fertilizer micro emulsion A micro emulsion in step (1) is sent in high speed lifting stirrer, add in proportion again step positively charged water-soluble polymer micro-emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add again a certain proportion of electronegative water-soluble polymer micro-emulsion, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1 ~ 2:1 ~ 2:1 ~ 2, utilizing pH adjusting agent to regulate pH value is 3.8 ~ 5.0, design temperature is 25 ℃ ~ 35 ℃, high-speed stirring, after mixing, there is aggregation in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in adding the Nano capsule of the solidifying agent gained in step (2) high speed lifting stirrer that accounts for A micro emulsion 2% ~ 10%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule moulding, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring static 10 ~ 20min;
(4), gained Nano capsule mixed solution in step (3) is washed twice with clear water, remove unreacted polymkeric substance and unnecessary solidifying agent, by pH adjusting agent, regulate pH value to 6.5 ~ 7.0, utilize whizzer centrifuging, spraying is dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
5. the preparation method of the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 4, it is characterized in that: wherein the polyvalent alcohol nonionic surface active agent described in step (1) is one or more following mixtures: sorbitol ester, tween, polyvinyl alcohol, sucrose fatty ester, diethanolamine fatty acid ester, methacrylic acid stearyl ester.
6. the preparation method of the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 4, it is characterized in that: wherein the pH adjusting agent described in step (2) and step (4) is acid-base modifier, wherein acidity regulator is: citric acid, oxalic acid, tartrate; Alkalinity regulator is sodium hydroxide solution.
7. the preparation method of the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 4, it is characterized in that: wherein the solidifying agent described in step (3) is one or more following mixtures: methacrylic acid imidazolidyl ketone hydroxyl ethyl ester, glutaraldehyde, Virahol, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2 isopropyl imidazole, diethyl amino propylamine, Triethylenetetramine (TETA), dimethylaminopropylamine.
8. the preparation method of the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 4, it is characterized in that: the wherein positively charged water-soluble polymer micro-emulsion described in step (2) and electronegative water-soluble polymer micro-emulsion, at chemical fertilizer micro emulsion A micro emulsion, there is aggregation around, coated core, forms Nano capsule.
9. the preparation method of the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 4, it is characterized in that: wherein the high pressure homogenizer described in step (1) is electromechanical type convection current high pressure homogenizer, in homogeneous chamber, be provided with two fluid channels, left and right, utilize distinctive Y-shaped structure, make the material convection current of high-pressure solution high speed motion from colliding, be ground into nanometer micro emulsion.
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